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DOE OSTI2025

Contrasting Chemical Kinetic Parameters for Near In‐Service‐Temperature Aging and High‐Temperature Thermal Decomposition of Triaminotrinitrobenzene Formulations

Triaminotrinitrobenzene-based high explosives such as LX-17 offer high energy density and exceptional safety, yet their long-term aging behavior at low temperatures remains poorly understood. In this study, several legacy and new production lots of LX-17 were subjected to accelerated aging experiments below 100°C, during which the formation rate of the initial degradation product, monofurazan (F1), was monitored. Kinetic analysis was performed using a sample-age-aware computational approach, yielding activation energy estimates of 82–91 kJ mol −1 for the low-temperature initiation step—markedly lower than the ∼200 kJ mol −1 associated with high-temperature thermal decomposition. Extrapolation from established cookoff models supports the conclusion that the dominant degradation mechanism at low temperatures differs from that at high temperatures. In conclusion, our results provide a unified kinetic framework that bridges the gap between in-service conditions and high-temperature damage.

Chemistry - Chemical explosives↗

DOE OSTI2018

Application of multiple-isotope and groundwater-age data to identify factors affecting the extent of denitrification in a shallow aquifer near a river in South Korea

The extent of denitrification in a small agricultural area near a river in Yangpyeong, South Korea, was determined using multiple isotopes, groundwater age, and physicochemical data for groundwater. The shallow groundwater at one monitoring site had high concentrations of NO{sub 3}-N (74–83 mg L{sup −1}). The δ{sup 15}N-NO{sub 3} values for groundwater in the study area ranged between +9.1 and +24.6‰ in June 2014 and +12.2 to +21.6‰ in October 2014. High δ{sup 15}N-NO{sub 3} values (+10.7 to +12.5‰) in both sampling periods indicated that the high concentrations of nitrate in the groundwater originated from application of organic fertilizers and manure. In the northern part of the study area, some groundwater samples showed elevated δ{sup 15}N-NO{sub 3} and δ{sup 18}O-NO{sub 3} values, which suggest that nitrate was removed from the groundwater via denitrification, with N isotope enrichment factors ranging between −4.8 and −7.9‰ and O isotope enrichment factors varying between −3.8 and −4.9‰. Similar δD and δ{sup 18}O values of the surface water and groundwater in the south appear to indicate that groundwater in that area was affected by surface-water infiltration. The mean residence times (MRTs) of groundwater showed younger ages in the south (10–20 years) than in the north (20–30 years). Hence, it was concluded that denitrification processes under anaerobic conditions with longer groundwater MRT in the northern part of the study area removed considerable amounts of nitrate. This study demonstrates that multi-isotope data combined with physicochemical data and age-dating information can be effectively applied to characterize nitrate contaminant sources and attenuation processes.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2019

Ageing and Its Influence on Vibration Characteristics of Jute/Polyester Composites

In this work, the influence of ageing on vibration characteristics of jute/polyester composite was investigated by varying the fiber length and weight percent. The ageing of composite was carried out under normal and seawater in room temperature. From the result, it is observed that the composite with the fiber length of 5 mm and 25-weight percentage has least moisture absorption and permeability than other types in both normal and seawater due to better fiber-matrix adhesion and closed pack arrangement of fibers. In addition, the above said combination shows better stability and vibration properties are least effected. Further, due to aging, the bonding between fiber and matrix is significantly affected to a larger degree with increase in the fiber content and length, which in turn decreases the natural frequency and damping properties of the composites.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Age-dating methodology for 137 Cs ceramic sources

Here, age-dating of 137 Cs ceramic sources is shown to be a viable technology for nuclear forensics investigations. The 137 Cs age-dating method in general, however, could be substantially improved by using radiometric rather than ICP-MS measurement of the 137 Cs isotope and by refining the Cs/Ba separation process. With these improvements, uncertainty in the age of a 60-year-old source decreases from 1.35 to 0.68 y.

137Cs ceramic↗

DOE OSTI2022

Elamipretide effects on the skeletal muscle phosphoproteome in aged female mice

The age-related decline in skeletal muscle mass and function is known as sarcopenia. Sarcopenia progresses based on complex processes involving protein dynamics, cell signaling, oxidative stress, and repair. We have previously found that 8-week treatment with elamipretide improves skeletal muscle function, reverses redox stress, and restores protein S-glutathionylation changes in aged female mice. This study tested whether 8-week treatment with elamipretide also affects global phosphorylation in skeletal muscle consistent with functional improvements and S-glutathionylation. Using female 6–7-month-old mice and 28–29-month-old mice, we found that phosphorylation changes did not relate to S-glutathionylation modifications, but that treatment with elamipretide did partially reverse age-related changes in protein phosphorylation in mouse skeletal muscle.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2018

High-Temperature Low-Cycle Fatigue Behavior of HS80H Ferritic–Martensitic Steel Under Dynamic Strain Aging

In this work, low-cycle fatigue tests were performed on HS80H ferritic–martensitic steel with the strain amplitudes ranging from 0.5 to 2.0% at room temperature and 350 °C. The cyclic stress response at 350 °C was found to be different from that at room temperature due to the effect of dynamic strain aging and showed a significant secondary hardening when the strain values were 0.5 and 0.7%. Furthermore, the dynamic strain aging effect also resulted in an abnormal increase in fatigue life when the strain was 0.7%, which was due to the change in elastic strain. Additionally, the elastic strain and fatigue life were bilinear relations in the double logarithmic coordinates. Finally, the transmission electron microscope observations showed that the dynamic strain aging led to the change in substructure, while the grain was refined.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Evolution of Crystallographic Structure of M{sub 23}C{sub 6} Carbide Under Thermal Aging of P91 Steel

The structural changes of P91 steel after different heat treatment and M{sub 23}C{sub 6} lattice expansion are well described by JMA kinetics law; however, the role of molybdenum on the M{sub 23}C{sub 6} lattice expansion is not clearly revealed. The aim of the present work is to investigate the solubility of molybdenum in M{sub 23}C{sub 6} lattice when iron or chromium atoms are replaced by molybdenum and to examine the effect of crystallographic structure changes on the mechanical properties of thermal aged P91 steel. Rietveld analysis of electrochemically extracted residues from the as-received and thermally aged at 600, 650 and 700 °C steel revealed that it is possible to measure and evaluate quantitatively the fraction of 8c crystallographic site occupation by molybdenum atoms of the M{sub 23}C{sub 6} lattice. It was shown that the value of the site occupation factor plotted in natural logarithmic scale increases linearly and obeys Johnson–Mehl–Avrami kinetic law, giving Avrami exponent n{sub avg} = 0.3356 and activation energy E = 272 kJ/mol. Hardness measurements of the aged samples indicate that the deterioration of properties is closely coherent to the growth of crystallite size.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Microstructures and Impact Wear Behavior of Al-Alloyed High-Mn Austenitic Cast Steel After Aging Treatment

The microstructural evolution and impact wear behavior of Al-alloyed ultra-high-Mn austenitic cast steel were investigated after different heat treatments, including quenching (Q) and quenching + aging (Q + A). Another ultra-high-Mn austenitic cast steel without Al was compared under the same experimental condition. After Q + A, Al addition contributed to the precipitation of κ-carbides which improves the yield strength and wear resistance of the austenite matrix. However, the mechanical properties and wear resistance of the Al-free steel were strongly deteriorated due to the precipitation of plate-like M{sub 3}C-type carbides, as well as the worn surface of the Al-free steel had the feature of micro-scratches. After Q + A (2 h), the Al-alloyed steel obtained optimal wear resistance and the main wear feature was strain fatigue. But, excessive aging time (4 h) would lead to a large fragile peeling from the worn surface and the wear resistance was decreased. Also, the worn subsurface microstructures with different heat treatments were observed by transmission electron microscopy (TEM). These results show that the deformation microstructures of the Al-free steel contained stacking faults, dislocation tangle and deformation twins. The deformation character of Al-alloyed steel is dominated by planar glide, and with increase in the aging time, planar dislocation substructures gradually evolved, relating to dislocation pileups, Taylor lattices and micro-bands.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Flow Directions and Ages of Subsurface Water in a Salt Marsh System Constrained by Isotope Tracing

Salt marshes are dynamic hydrologic systems where terrestrial groundwater, terrestrial surface water, and seawater mix due to bi-directional flows and pressure gradients. Due to the counteracting terrestrial and marine forcings that control these environments, we do not comprehensively understand water fluxes in these complex coastal systems. To understand the water sources, flow directions, and velocities in salt marsh porewater, we employed a combination of geochemical tracers and analytical models across a hillslope-to-salt marsh continuum in a salt marsh experiencing daily inundation of estuarine surface water (SW) from tides and mixing of fresh seasonal groundwater. We used tritium ( 3 H) as a hydrologic tracer to assess porewater ages and stable water isotope ($\delta$ 2 H and $\delta$ 18 O) analyses to separate isotopically distinct estuarine and terrestrial groundwater across different depths and landscape positions in the study transect. We employed electrical conductivity to constrain the role of source mixing and evapotranspiration in salt marsh hydrology. Salinity and stable isotopes revealed that transpiration, rather than evaporation, increased subsurface water salinity to concentrations above estuarine SW during summer. Elevated salinity at depth indicated that salt marsh subsurface water is recharged during the dry growing season. Seasonal recharge patterns drive long-term deep subsurface water dynamics across the salt marsh, with 3 H ages of 3–7 years, and daily tidal cycles drive short-term shallow porewater dynamics with 3 H ages of 0 ± 3.6 years. Furthermore, our conceptual understanding of the spatiotemporal changes in SW-subsurface water interactions at the terrestrial-marine interface quantifies the hydrological constraints we are missing to improve our understanding of biogeochemical cycles within the salt marsh.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

High strain rate deformation of aged TRIP Ti-10V-2Fe-3Al (wt.%) examined by in-situ synchrotron X-ray diffraction

Transformation Induced Plasticity (TRIP) is a promising avenue for tailoring the work hardening response of metastable $β$ titanium (Ti) alloys. Here we show that aged TRIP Ti-10V-2Fe-3Al (wt.%) maintains higher elongations and flow stresses as strain rate increases, if phase stability and microstructural characteristics are tuned. Low temperature aging influences the matrix $β$ phase stability by $ω$ phase precipitation, which affords a promising way to impact the TRIP effect and obtain desirable mechanical properties, ranging from high damping capacity to good strength/ductility combinations. Although TRIP is active during quasi-static and dynamic testing up to 2000 s –1 , increasing aging time and/or strain rate reduces the overall propensity for the TRIP effect and extent of transformation, which occurs rapidly just at the onset of yielding. Importantly, TRIP with $ω$ phase precipitation provides interesting alloying, microstructure, and property design strategies for engineering applications like lightweight protective structures, where high strains and the need for energy absorption are encountered.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Impact of changes in protective behaviors and out-of-household activities by age on COVID-19 transmission and hospitalization in Chicago, Illinois

Even with an efficacious vaccine, protective behaviors (social distancing, masking) are essential for preventing COVID-19 transmission and could become even more important if current or future variants evade immunity from vaccines or prior infection. Here we created an agent-based model representing the Chicago population and conducted experiments to determine the effects of varying adult out-of-household activities (OOHA), school reopening, and protective behaviors across age groups on COVID-19 transmission and hospitalizations. From September-November 2020, decreasing adult protective behaviors and increasing adult OOHA both substantially impacted COVID-19 outcomes; school reopening had relatively little impact when adult protective behaviors and OOHA were maintained. As of November 1, 2020, a 50% reduction in young adult (age 18-40) protective behaviors resulted in increased latent infection prevalence per 100,000 from 15.93 (IQR 6.18, 36.23) to 40.06 (IQR 14.65, 85.21)and 19.87 (IQR 6.83, 46.83) to 47.74 (IQR 18.89, 118.77) with 15% and 45% school reopening. Increasing adult (age ≥18) OOHA from 65% to 80% of pre-pandemic levels resulted in increased latent infection prevalence per 100,000 from 35.18 (IQR 13.59, 75.00) to 69.84 (IQR 33.27, 145.89) and 38.17 (IQR 15.84, 91.16) to 80.02 (IQR 30.91, 186.63) with 15% and 45% school reopening. Similar patterns were observed for hospitalizations. In areas without widespread vaccination coverage, interventions to maintain adherence to protective behaviors, particularly among younger adults and in out-of-household settings, remain a priority for preventing COVID-19 transmission.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2011

Senescence marker protein 30 (SMP30)/regucalcin (RGN) expression decreases with aging, acute liver injuries and tumors in zebrafish

Highlights: {yields} Zebrafish SMP30/RGN mRNA expression decreases with aging. {yields} Decreased expression was observed in liver tumors as compared to the surrounding area. {yields} SMP30/RGN is important for liver proliferation and tumorigenesis. -- Abstract: Senescence marker protein 30 (SMP30)/regucalcin (RGN) is known to be related to aging, hepatocyte proliferation and tumorigenesis. However, expression and function of non-mammalian SMP30/RGN is poorly understood. We found that zebrafish SMP30/RGN mRNA expression decreases with aging, partial hepatectomy and thioacetamide-induced acute liver injury. SMP30/RGN expression was also greatly decreased in a zebrafish liver cell line. In addition, we induced liver tumors in adult zebrafish by administering diethylnitrosamine. Decreased expression was observed in foci, hepatocellular carcinomas, cholangiocellular carcinomas and mixed tumors as compared to the surrounding area. We thus showed the importance of SMP30/RGN in liver proliferation and tumorigenesis.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2023

Perovskite evolution on La modified Mn 1.5 Co 1.5 O 4 spinel through thermal ageing with enhanced oxidation activity: Is sintering always an issue?

Non-precious metal oxides have great potential in catalytic deep oxidation of emitted hydrocarbons to help address various environmental pollution concerns. However, sintering issue is a stumbling block in practical application upon long-term high-temperature operation or thermal shock experience. Herein, La was applied to modify Mn 1.5 Co 1.5 O 4 spinel to get a highly active oxidation catalyst with exceptional stability against high-temperature thermal ageing treatment. With thermal ageing at 750 °C for 100 h, the La modified Mn–Co composite reached 90 % conversion in toluene oxidation at 265 °C under the high WHSV of 120,000 mL g -1 h -1 , while this value increased to 312 °C over blank Mn–Co spinel. The addition of La not only inhibited the growth of spinel nanocrystals, but also brought about perovskite formation through sintering, generating perovskite-spinel interfaces, thus enhancing both activity and stability. Meanwhile, the La modified Mn–Co spinel exhibited superior performance in presence of water or sulfur dioxide after thermal ageing treatment. In conclusion, this work offers a versatile strategy to design anti-sintering and active oxidation nanocatalysts based on non-precious metal oxides for industrial applications.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Effects of Sn addition on precipitation of Al–Zn–Mg alloy at early stage of natural aging

The effect of Sn addition on the natural aging behavior of Al–Zn–Mg alloy was investigated using atom probe tomography (APT) experiments and density functional theory (DFT) calculations. The results demonstrate that Sn retards the natural aging behavior by facilitating the preferential formation of Mg–Sn clusters, which suppress the formation of Guinier-Preston zones (I) during the earliest aging stage. Quantitative solute analysis conducted by APT has suggested increasing amount of Mg–Sn clusters in Sn-contained alloy due to their high binding energy, supported by DFT calculations on the Sn.

36 MATERIALS SCIENCE↗

DOE OSTI2024

New insights on the effects of chemistry and temperature on α’ precipitation during aging of FeCrAl alloys

Here, the effect of Al on α' precipitation in FeCrAl alloys was studied through thermal aging of several model binary FeCr and FeCrAl alloys with Cr content of 13 wt.%, 17 wt.%, and 25 wt.% with and without 5.5 wt.% Al. Aging was performed up to 1,000h at varying temperatures from 400-500°C. At 400°C no age hardening was observed due to slow kinetics at this temperature. For both the 17Cr and 25Cr alloys, the addition of Al shows a lowering of the miscibility gap, consistent with other reports in literature. Interestingly, however, for the 25Cr alloys the addition of Al in the FeCrAl ternary alloy accelerated α' precipitation below the miscibility gap. Such enhanced precipitation has also been predicted by our atomistic kinetic Monte Carlo (AKMC) simulations. While previous literature has often focused on Al suppressing α', here we show that while Al can lower the miscibility gap in the Fe-Cr ferritic system thermodynamically, it may also enhance the kinetics of precipitation.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Binder characterisation of mortars used at different ages in the San Lorenzo church in Milan

The paper describes a study on the mortars of the basilica of San Lorenzo in Milan, which was carried out to support an archaeological study aimed at dating and documenting the construction techniques used throughout the centuries. The church, which was founded between the 4th and 5th century, at the end of the period when Milan was the capital of the Roman Empire, was subjected in time to extensions, collapses and reconstructions that lasted until the Renaissance period and even later on. Thanks to the good state of conservation, San Lorenzo church is a collection of materials and construction techniques throughout a period of more than a millennium. Mortars were investigated in order to compare the binders used for structural elements built in different historical ages. From an archaeological study, samples of mortars attributed to the late Roman period, the Middle Ages and the Renaissance were available. The binder of each sample was separated by the aggregates and it was characterised on the basis of X-ray diffraction analysis, thermogravimetric analysis and scanning electron microscopy. Constituents of the binder were identified and their origin is discussed in order to investigate if they could be attributed to the original composition of the binder or to possible alteration in time due to atmospheric pollution. Results show that, even though the binder is mainly based on magnesian lime, there are significant differences in the microstructure of the binding matrix used in mortars ascribed to the different historical periods. In the Roman period, in correspondence of the structural elements that required higher strength, also hydraulic cocciopesto mortars were detected. Gypsum was found in most samples, which was maybe added intentionally. - Highlights: • Binders of mortars of San Lorenzo church in Milan were investigated. • Roman, Middle Ages and Renaissance samples were studied by XRD, TG and SEM. • Magnesian-lime binders containing silico-aluminates were used in all periods. • Cocciopesto hydraulic mortars were used only in the Roman period. • Gypsum was found in most samples, which was maybe added intentionally.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Precipitation behavior of stainless steel weld overlay cladding exposed to a long-term thermal aging

Highlights: • Silicide phase formation with G-phase was first time to be observed. • Precipitation behavior discrepancy existed at different locations of ferrite phase. • G-phase and silicide phase formed along dislocations and within ferrite matrix. • Heterogeneous distribution of elements induced silicide phase formation. - Abstract: Thermal aging behavior of stainless steel weld overlay cladding aged at 400 °C for 10,000 h was investigated. The results showed that the precipitates along the dislocation and within ferrite matrix contained the face-centered cubic structural G-phase and silicide phase. Silicide phase, supposed to be (Fe, Mn){sub 3}Si phase, preferred to form with G-phase along the dislocations and within ferrite matrix. Silicide phase showed a cube-on-cube relationship with ferrite phase and G-phase. Heterogeneous distribution of elements within Ni-Mn-Si clusters was responsible for silicide phase formation during thermal aging process, and the corresponding precipitation behavior discrepancy at different forming sites (dislocations, ferrite matrix and phase boundary) was discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Extended investigation of sol aging effect on TiO2 electron transporting layer and performances of perovskite solar cells

Highlights: • Conditions of deposition of compact sol-gel TiO{sub 2} significantly influence the parameters of perovskite cells. • Sol aging originally considered as beneficial was proved to be adverse due to no repeatability, defects and residual water. • Free from such disadvantages TiO{sub 2} made from fresh sol can support as good cell parameters. • Roughness of transparent conductive oxide influences the optimal thickness of electron transporting layer. - Abstract: Organic−inorganic hybrid perovskites have created significant opportunities for low-cost and high-performance solar cells. The electron transporting layer (ETL) is one of the main components of the solar cell, which selectively transports electrons and at the same time acts as a barrier for holes. This paper focuses on the ETL composed of titanium dioxide deposited by sol-gel method. In particular, perovskite solar cells with ETL from aged titanium sol revealed significant differences of short circuit current which is 8% higher than their counterpart with ETL from fresh sol. Analysis of ETL morphology by atomic force microscopy combined with electrochemical impedance spectroscopy and optical properties measurements enabled to determine the source of this diversity. Additionally, the role of roughness of transparent electrode was indicated. The in-depth material analysis revealed some disadvantages of the ETL material, originally considered as supporting higher photovoltaic performance. The results indicated several problems associated with hardly controlled aging conditions, defects and presence of residual water, strongly advocate for TiO{sub 2} ETL form the fresh sol, which after optimization can guarantee the same good solar cell performance.

14 SOLAR ENERGY↗